5,6-dichloro-3,4-dihydro-2H-naphthalen-1-one

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Polyphosphoric acid (35 g) was heated to melt at 120 C for 30 minutes. To this was added 1.2 g (5.1 mmol) 4-(2,3-dichlorophenyl)butanoic acid (PC68) and this mixture was heated further with stirring for 10 h at 130 C. LCMS analysis showed the formation of the product and the disappearance of starting material. The reaction mixture was then cooled and water (100 ml) was added. It was then extracted with ethylacetate (100 ml) and then was washed with Saturated Sodium bicarbonate (50 ml). The organic phase was dried and evaporated in vacuum. The oily residue was subjected to column chromatography with Hexane-ethylacetate (98:2) to obtain the tetralone as a yellow solid. this mixture was heated further The reaction mixture was then cooled It was then extracted with ethylacetate (100 ml) was washed with Saturated Sodium bicarbonate (50 ml) The organic phase was dried evaporated in vacuum

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Polyphosphoric acid (35 g) was heated to melt at 120 C for 30 minutes. To this was added 1.2 g (5.1 mmol) 4-(2,3-dichlorophenyl)butanoic acid (PC68) and this mixture was heated further with stirring for 10 h at 130 C. LCMS analysis showed the formation of the product and the disappearance of starting material. The reaction mixture was then cooled and water (100 ml) was added. It was then extracted with ethylacetate (100 ml) and then was washed with Saturated Sodium bicarbonate (50 ml). The organic phase was dried and evaporated in vacuum. The oily residue was subjected to column chromatography with Hexane-ethylacetate (98:2) to obtain the tetralone as a yellow solid. this mixture was heated further The reaction mixture was then cooled It was then extracted with ethylacetate (100 ml) was washed with Saturated Sodium bicarbonate (50 ml) The organic phase was dried evaporated in vacuum